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US3714097A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing low foaming latexes of interpolymers containing vinyl chloride and ethylene

Assignee: Goodrich Corp
•
Filing: 1970-06-08
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Granted: 1973-01-30
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Expires: 1990-06-08
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Abstract

Abstract This invention relates to stable vinyl chloride/ethylene interpolymer latexes polymerized at between about 50 and 15,000 psi., which latexes can be removed from said reactors without the usual venting difficulties of foaming, coagulation and valve clogging. The method of making said latexes comprises gradually adding comonomer including a major proportion of vinyl chloride over a period of at least six hours, to an aqueous composition maintained under ethylene pressure and containing a seed latex, a free-radical initiating system and an amount of emulsion stabilizer below that which will cause substantial foaming.

Inventors

  • 👤 P Cautilli
  • 👤 S Makower

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 08:51
CPC Classifications
C; C08; C08F; C08F214/00; C08F214/02; C08F214/04; C08F214/06; C08F291/00

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 131 words
In the emulsion-polymerization at superatmospheric pressure of an interpolymer comprising vinyl chloride and ethylene, an improvement which provides a stable latex product that remains mechanically stable during and after release of said pressure, said improvement comprising the sequential steps of a. maintaining ethylene pressure at a level between about 50 and 15,000 psi on an aqueous composition containing i. a seed latex made by free-radical initiated emulsion copolymerization of ethylenically unsaturated monomers, ii. an anionic surfactant in amount at least 0.005 percent and not exceeding 0.4 percent based on weight of comonomer charged, and iii. a free-radical initiator system maintained at a level sufficient to effect emulsion polymerization while b. adding gradually, over a period of not less than six hours, a comonomer charge including a major proportion of vinyl chloride.
Claim 2
Dependent Claim 131 words
In the emulsion-polymerization at superatmospheric pressure of an interpolymer comprising vinyl chloride and ethylene, an improvement which provides a stable latex product that remains mechanically stable during and after release of said pressure, said improvement comprising the sequential steps of a. maintaining ethylene pressure at a level between about 50 and 15,000 psi on an aqueous composition containing i. a seed latex made by free-radical initiated emulsion copolymerization of ethylenically unsaturated monomers, ii. an anionic surfactant in amount at least 0.005 percent and not exceeding 0.4 percent based on weight of comonomer charged, and iii. a free-radical initiator system maintained at a level sufficient to effect emulsion polymerization while b. adding gradually, over a period of not less than six hours, a comonomer charge including a major proportion of vinyl chloride.
Claim 3
Dependent Claim 23 words
The improvement of claim 1 wherein the surfactant is selected from the group consisting of sodium lauryl sulfate and sodium dodecyl benzene sulfonate.
Claim 4
Dependent Claim 42 words
The improvement of claim 1 wherein the seed latex has a particle size between about 0.005 and 0.10 microns and is present in an amount between about 0.01 percent and 10 percent solids based on the total amount of said comonomer charge.
Claim 5
Dependent Claim 12 words
The improvement of claim 1 wherein all the comonomer is vinyl chloride.
Claim 6
Dependent Claim 45 words
The improvement of claim 1 wherein the minor proportion of comonomer is selected from the group consisting of vinyl acetate, vinyl propionate, vinylidene chloride, propylene, butene, and esters of acrylic or methacrylic acid with alkanols containing up to ten carbon atoms in the alkyl group.
Claim 7
Dependent Claim 16 words
The improvement of claim 1 wherein the temperature of interpolymerization is between about 15*C and 85*C.
Claim 8
Dependent Claim 41 words
The improvement of claim 1 wherein the pressure is maintained at a level between about 500 and 3,000 psi, the temperature of interpolymerization is between about 50*C and 85*C, and the initiator system is a water-soluble alkali metal persulfate or peroxydiphosphate.
Claim 9
Dependent Claim 122 words
An emulsion polymerization method of preparing a stable latex of a copolymer containing between about 70- 94 percent of vinyl chloride and correspondingly 30-6 percent ethylene, said method comprIsing a. maintaining ethylene pressure at between about 500 and 3,000 psi on an aqueous composition at a temperature between about 50*C and 85*C, said aqueous composition containing a seed latex, an anionic surfactant in amount at least 0.005 percent and not exceeding 0.4 percent based on weight of the vinyl chloride added, and an initiator selected from the group consisting of water-soluble persulfates and peroxydiphosphates, said initiator being maintained at a level sufficient to effect polymerization while b. adding vinyl chloride monomer gradually over a period of not less than about 6 hours.
Claim 10
Dependent Claim 122 words
An emulsion polymerization method of preparing a stable latex of a copolymer containing between about 70- 94 percent of vinyl chloride and correspondingly 30-6 percent ethylene, said method comprIsing a. maintaining ethylene pressure at between about 500 and 3,000 psi on an aqueous composition at a temperature between about 50*C and 85*C, said aqueous composition containing a seed latex, an anionic surfactant in amount at least 0.005 percent and not exceeding 0.4 percent based on weight of the vinyl chloride added, and an initiator selected from the group consisting of water-soluble persulfates and peroxydiphosphates, said initiator being maintained at a level sufficient to effect polymerization while b. adding vinyl chloride monomer gradually over a period of not less than about 6 hours.
Claim 11
Independent Claim 127 words
A method of preparing by emulsion polymerization a stable latex of a terpolymer of vinyl chloride, vinyl acetate and ethylene which comprises maintaining ethylene pressure at between about 500 psi and 3,000 psi on an aqueous composition at a temperature between about 50*C and 85*C, said aqueous composition containing a seed latex and an anionic surfactant in an amount between about 0.005 percent and about 0.4 percent based on total weight of vinyl chloride and vinyl acetate added; adding gradually thereto over a period of between about 6 and 24 hours an aqueous solution of a water-soluble alkali metal persulfate or peroxydiphosphate to effect polymerization while simultaneously adding over the same period both vinyl chloride and vinyl acetate in the weight proportions between about 51/49 and 99/1.
Claim 12
Independent Claim 127 words
A method of preparing by emulsion polymerization a stable latex of a terpolymer of vinyl chloride, vinyl acetate and ethylene which comprises maintaining ethylene pressure at between about 500 psi and 3,000 psi on an aqueous composition at a temperature between about 50*C and 85*C, said aqueous composition containing a seed latex and an anionic surfactant in an amount between about 0.005 percent and about 0.4 percent based on total weight of vinyl chloride and vinyl acetate added; adding gradually thereto over a period of between about 6 and 24 hours an aqueous solution of a water-soluble alkali metal persulfate or peroxydiphosphate to effect polymerization while simultaneously adding over the same period both vinyl chloride and vinyl acetate in the weight proportions between about 51/49 and 99/1.
Claim 13
Independent Claim 184 words
A method of preparing by emulsion polymerization a latex containing between about 40 percent and 66 percent solids of a vinyl chloride/ethylene copolymer comprising about 17-20 percent by weight ethylene, said method comprising the steps of a. maintaining substantially constant ethylene pressure at between about 1,200 and 1,500 psi on an aqueous composition at a temperature of between about 55*C and 70*C, said composition comprising between about 0.5 percent and 3.0 percent of a polyvinyl chloride or poly (2-ethyl hexyl acrylate) seed latex and between about 0.005% and about 0.4 percent of an anionic surfactant, b. adding gradually thereto at a substantially constant rate, over a period of between about 12-16 hours, an aqueous solution of a persulfate or peroxydiphosphate initiator, in an amount between about 0.2 percent and 2 percent based on weight of the aqueous composition, to effect polymerization while c. simultaneously adding gradually over the same period an amount of vinyl chloride in about 5-20 percent excess over the theoretical amount needed to obtain the expected solids and d. maintaining the polymerizing system at 55*-70*C until the required solids is obtained.
Claim 14
Independent Claim 184 words
A method of preparing by emulsion polymerization a latex containing between about 40 percent and 66 percent solids of a vinyl chloride/ethylene copolymer comprising about 17-20 percent by weight ethylene, said method comprising the steps of a. maintaining substantially constant ethylene pressure at between about 1,200 and 1,500 psi on an aqueous composition at a temperature of between about 55*C and 70*C, said composition comprising between about 0.5 percent and 3.0 percent of a polyvinyl chloride or poly (2-ethyl hexyl acrylate) seed latex and between about 0.005% and about 0.4 percent of an anionic surfactant, b. adding gradually thereto at a substantially constant rate, over a period of between about 12-16 hours, an aqueous solution of a persulfate or peroxydiphosphate initiator, in an amount between about 0.2 percent and 2 percent based on weight of the aqueous composition, to effect polymerization while c. simultaneously adding gradually over the same period an amount of vinyl chloride in about 5-20 percent excess over the theoretical amount needed to obtain the expected solids and d. maintaining the polymerizing system at 55*-70*C until the required solids is obtained.
Claim 15
Dependent Claim 169 words
A stable latex having a solids content of between about 40 percent and 66 percent, of a vinyl chloride/ethylene copolymer containing about 17-20 percent ethylene, made by an emulsion polymerization method comprising the steps of a. maintaining substantially constant ethylene pressure at between about 1,200 and 1,500 psi of an aqueous composition at a temperature of about 55*-70*C, said composition containing between about 0.5 percent and 3.0 percent of a poly (2-ethyl hexyl acrylate) seed latex and at least about 0.005 percent and not more than about 0.4 percent of an anionic surfactant, b. adding gradually thereto at a substantially constant rate, over a period of between about 12-16 hours, an aqueous solution of a water-soluble alkali metal persulfate or peroxydiphosphate, in an amount to effect polymerization while c simultaneously adding gradually over the same period an amount of vinyl chloride in about 5-20 percent excess over the theoretical amount needed to obtain the expected solids, and d. maintaining thE polymerizing system at 55*-70*C until required solids is obtained.
Claim 16
Dependent Claim 169 words
A stable latex having a solids content of between about 40 percent and 66 percent, of a vinyl chloride/ethylene copolymer containing about 17-20 percent ethylene, made by an emulsion polymerization method comprising the steps of a. maintaining substantially constant ethylene pressure at between about 1,200 and 1,500 psi of an aqueous composition at a temperature of about 55*-70*C, said composition containing between about 0.5 percent and 3.0 percent of a poly (2-ethyl hexyl acrylate) seed latex and at least about 0.005 percent and not more than about 0.4 percent of an anionic surfactant, b. adding gradually thereto at a substantially constant rate, over a period of between about 12-16 hours, an aqueous solution of a water-soluble alkali metal persulfate or peroxydiphosphate, in an amount to effect polymerization while c simultaneously adding gradually over the same period an amount of vinyl chloride in about 5-20 percent excess over the theoretical amount needed to obtain the expected solids, and d. maintaining thE polymerizing system at 55*-70*C until required solids is obtained.

References Cited (Backward Citations)

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1976-01-30 1976-07-31 1977-01-30 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1980-01-30 1980-07-31 1981-01-30 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1984-01-30 1984-07-31 1985-01-30 $7700.00 Window Closed / Lapsed

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